Water → 5,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

HRID 569807

반응식

HRID 569807 반응식
[Cl:1][C:2]1[CH:10]=[C:9]([Cl:11])[CH:8]=[C:7]2[C:3]=1[C:4](=[O:13])[C:5](=[O:12])[NH:6]2.[OH2:14]>C(O)(=O)C.[O-2].[O-2].[O-2].[Cr+6]>[Cl:1][C:2]1[C:3]2[C:4](=[O:13])[O:12][C:5](=[O:14])[NH:6][C:7]=2[CH:8]=[C:9]([Cl:11])[CH:10]=1

참가 물질

5

반응물 2

HCID 962WaterHCID 2519084,6-Dichloroisatin

생성물 1

HCID 123632155,7-dichloro-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione

시약·촉매·용매 2

HCID 10219390chromium (VI) trioxide촉매HCID 176Acetic Acid용매

실험 절차

To a suspension of 4,6-dichloroindolin-2,3-dione (5.95 g) in acetic acid (95 ml) was added chromium trioxide (16 g) over a period of 15 minutes at 60° C. with stirring and the mixture was stirred at 70°-75° C. for 1 hour. After cooling, the reaction mixture was poured into water (360 ml) and the resulting precipitates were collected by filtration. The filtrate was extracted with ethyl acetate. The extract was washed with water and dried. Removal of the solvent gave a residue, which was combined with the precipitates. Recrystallization from isopropyl ether gave 5,7-dichloro-2H-3,1-benzoxazine-2,4(1H)-dione (2.85 g).

후처리

  1. stirringthe mixture was stirred at 70°-75° C. for 1 hour
  2. temperatureAfter cooling
  3. customthe resulting precipitates
  4. filtrationwere collected by filtration
  5. extractionThe filtrate was extracted with ethyl acetate
  6. washThe extract was washed with water
  7. customdried
  8. customRemoval of the solvent
  9. customgave a residue, which
  10. customRecrystallization from isopropyl ether

출처 및 근거

ORD 기록
ord-96b79913e52e4204b7065cc2cf9372a3
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04734419

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